CN104893009B - A kind of starch-based composite material and preparation method - Google Patents
A kind of starch-based composite material and preparation method Download PDFInfo
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Abstract
The invention discloses a kind of starch-based composite material and preparation methods.Composite material is blended by modified starch and polyester melt, 100 parts by weight of modified starch, and polyester is 10~100 parts by weight；The general structure of the modified starch are as follows:Wherein St is starch molecule, and R group is alkyl (CnH2n+1).The esterification starch is prepared by the following components of parts by weight meter: 100 parts of native starch, 0~200 part of solvent, 10~50 parts of catalyst, 1~50 part of modifying agent.Preparation method includes: that by the dosage melt blending starch-based composite material is made in the component.Invention has the advantages of high efficiency, at low cost, and simple process, performance is controllable, suitable for preparing the thermoplastic material of various performance requirements.
Description
Technical field
The present invention relates to starch technical fields, further say, are to be related to a kind of starch-based composite material and preparation method.
Background technique
China is a grain big country, annual to remove edible consumption and grain for industrial uses, also accumulates number in terms of 100,000 tons
Grain, according to national food sanitary standard, the grain for storing over 1 year is grain in storage for years, and the grain more than 3 years is grain in storage for years,
These grains neither able person's food cannot function as feed again, thus cause a large amount of waste.Part crop such as cassava, pueraria lobata simultaneously
Deng due to nutritive value it is low, be normally used for the industrial production of the low values high pollution such as papermaking, mortar.As a kind of natural polymer
Son, starch have the characteristics that it is renewable, degradable, cheap, easily deposit and be readily transported, if can be by grain in storage for years and low nutrition, low price
It is worth the Material Field of the starch application in crop, for improving crops added value, raising farmers' income reduces white pollution,
It develops a circular economy etc. and to be of great significance, be a new way for solving agriculture, rural areas and farmers.
Starch-based degradable plastics refer to the biodegradable plastic in its component containing starch or derivatives thereof.It is common to form sediment
Powder diameter is 25 μm or so, can not only be used for a kind of filler for preparing degrading composite, and can pass through certain modification system
Standby degradative plastics.Current most starch Biocomposite material is mainly open by preparing in starch filled high molecular method
Number CN102121199A proposes the preparation of starch filled artificial leather, and publication number CN101805463A proposes starch filled polypropylene
Preparation etc..Starch is filled as filler into nondegradable plastics, and damage type degradative plastics is made, after the plastics use,
Starch is degraded first, plastics is divided into fractionlet, but due to the presence of nondegradable plastics, this kind of plastics cannot be in the short time
It is interior degradable, it not can solve its harm to environment.Therefore nowadays the starch plastics for capableing of complete biodegradable, which become, to be ground
The main target studied carefully.
Publication number CN103554368A, which is proposed, to be modified starch and is applied in rubber, this is modified starch
The method applied afterwards can improve starch-based material performance, but there is starch distribution unevenness, it is bad with material compatibility
Problem.
Since starch does not have thermoplasticity, it is thus proposed that public by the thinking of elasticizer plasticizing starch then filled plastics
The patents such as the number of opening CN103146032A are blended with material in this way.Although this method part solves the heat of material
Modeling problem and the dispersion, but since the plasticizer of small molecule is easy to migrate, material property is deteriorated rapidly after migration, and due to increasing
The addition of agent is moulded, the water resistance of material can sharply decline, thus the performance of material is difficult to stablize.
Starch-based bio material at this stage, it is strong to solve hydrophily, mechanical property and the migration of plasticizer these three ask
The balance of topic, thus it is difficult to large-scale application.
Summary of the invention
To solve the problem in the prior art, the present invention provides a kind of starch-based composite material and preparation methods.
High-efficient, at low cost, simple process, performance is controllable, suitable for preparing the thermoplastic material of various performance requirements.
An object of the present invention is to provide a kind of starch-based composite material.
The composite material is blended by modified starch and polyester melt, 100 weight of modified starch in composite material
Part, 10~100 parts by weight of polyester；
The general structure of the modified starch are as follows:
Wherein St is starch molecule, and R group is alkyl (CnH2n+1), alkenyl (CnH2n), phenyl (CnHN~1) at least one
Kind, wherein n=2~18, R group are preferably alkyl (CnH2n+1)。
The esterification starch is prepared by the following components of parts by weight meter:
100 parts of native starch, 150~200 parts of solvent, 10~30 parts of catalyst, 1~20 part of modifying agent；
The native starch raw material is selected from cornstarch, tapioca, starch from sweet potato, potato starch, wheat starch, beans
At least one of kind of starch or sorghum starch；
The solvent is esters；Preferably at least one of ethyl acetate, butyl acetate, methyl acetate；
The catalyst is selected from organic bases or polyamine；Preferably in pyridine, pyrroles, ethylenediamine and triethylamine extremely
Few one kind；
The modifying agent is acyl chloride, preferably acryloyl chloride.
The modified starch is prepared by the method comprised the steps of:
(1) it the catalytic pretreatment of starch: is added in the obtained starch suspension of solvent and is added dropwise to native starch or native starch
Then catalyst stirs 0.5~3 hour at 10 DEG C~60 DEG C；
(2) modification of starch: being added dropwise modifying agent while stirring, and nothing is added after stirring 0.5~3 hour at 10 DEG C~60 DEG C
Water-ethanol washing filters, the modified starch is made after drying.
The polyester is preferably degradable polyester, such as polylactic acid (PLA), polycaprolactone (PCL), poly butylene succinate
(PBS), polyadipate/butylene terephthalate (PBAT), poly-β-hydroxybutyric acid (PHB), polyhydroxyalkanoate (PHA) etc..
The second object of the present invention is to provide a kind of preparation method of starch-based composite material.
Include:
The starch-based composite material is made by the dosage melt blending in the component.
It specifically includes:
Modified starch and polyester are passed through into two-roll mill or torque according to weight at 60~230 DEG C first
Rheometer or screw extruder melt blending 5~25 minutes are uniformly mixed and obtain blend.
30~200 revs/min of the torque rheometer rotor speed, preferably 50~100 revs/min.
80~300 revs/min of the screw extruder revolving speed, preferably 100~200 revs/min.
Compared to traditional starch filled thermoplastic material, the basic ideas of this method are the high reaction activities by acyl chlorides
Hydroxyl on substituted starch, can improve the hydrophily of starch by this method, while improve starch molecule and polyester material
This modified starch is carried out melt blending with polyester material and is made by the compatibility of material.
It is in order to measure the performance of material, composite material hot pressing obtained is in blocks, mechanics properties testing is carried out to material.Root
According to preparation method provided by the invention thermoplastic material obtained have biomass content is high, resilience is good, biodegradable,
The features such as thermoplastic property is excellent.A kind of starch-based composite material of the invention can realize on traditional simple synthesis device,
Industrialized production at low cost, environmental-friendly, easy to accomplish.
Specific embodiment
Below with reference to embodiment, the present invention is further illustrated.
Comparative example 1
By 100 parts of cornstarch (production of Changchun great achievement corn development corporation, Ltd.) and polycaprolactone (PCL) (Shenzhen brilliance
The production of great achievement Co., Ltd) 10 parts be uniformly mixed, pre-composition is placed in torque rheometer, and (Ha Bo Co., Ltd prepares RM-200
Type) in, 10min is blended in 50rpm at 70 DEG C.By blend, hot pressing is in blocks at 70 DEG C, is cut into batten according to national regulations and carries out
Mechanics Performance Testing.Test result is shown in Table 1.The water absorption rate in one week of test material, test result are included in table 1.
Comparative example 2
By 100 parts of tapioca (production of Shanghai Food Co., Ltd's today) and polyadipate/butylene terephthalate
(PBAT) 30 parts of (production of Shenzhen brilliance great achievement Co., Ltd) is uniformly mixed, and pre-composition is placed in torque rheometer and (wins limited in Kazakhstan
Corporation is for RM-200 type) in, 10min is blended in 50rpm at 70 DEG C.By blend, hot pressing is in blocks at 70 DEG C, advises according to national standard
Surely it is cut into batten and carries out Mechanics Performance Testing.Test result is shown in Table 2.The water absorption rate in one week of test material, test result are included in
In table 1.
Comparative example 3
By 100 parts of starch from sweet potato (production of Shanghai Food Co., Ltd's today) and (Shenzhen poly butylene succinate (PBS)
The production of brilliance great achievement Co., Ltd) 80 parts be uniformly mixed, pre-composition is placed in torque rheometer, and (Ha Bo Co., Ltd prepares RM-
200 types) in, 10min is blended in 50rpm at 70 DEG C.By blend, hot pressing is in blocks at 70 DEG C, according to national regulations be cut into batten into
Row Mechanics Performance Testing.Test result is shown in Table 2.The water absorption rate in one week of test material, test result are included in table 1.
Comparative example 4
By 100 parts of soybean starch (production of Shanghai Food Co., Ltd's today) and poly-β-hydroxybutyric acid (PHB) (Shenzhen brilliance
The production of great achievement Co., Ltd) 100 parts be uniformly mixed, pre-composition is placed in torque rheometer, and (Ha Bo Co., Ltd prepares RM-200
Type) in, 10min is blended in 50rpm at 70 DEG C.By blend, hot pressing is in blocks at 70 DEG C, is cut into batten according to national regulations and carries out
Mechanics Performance Testing.Test result is shown in Table 2.The water absorption rate in one week of test material, test result are included in table 1.
Comparative example 5
By 100 parts of soybean starch (production of Shanghai Food Co., Ltd's today) and polyhydroxyalkanoate (PHA) (Shenzhen light
The production of magnificent great achievement Co., Ltd) 10 parts be uniformly mixed, pre-composition is placed in torque rheometer, and (Ha Bo Co., Ltd prepares RM-200
Type) in, 10min is blended in 50rpm at 70 DEG C.By blend, hot pressing is in blocks at 70 DEG C, is cut into batten according to national regulations and carries out
Mechanics Performance Testing.Test result is shown in Table 2.The water absorption rate in one week of test material, test result are included in table 1.
The preparation of modified starch:
Modified starch 1: pyridine (traditional Chinese medicines collection is added dropwise to cornstarch (production of Changchun great achievement corn development corporation, Ltd.) 100g
The production of chemical reagent Co., Ltd, group) 10 parts, after being added dropwise to complete, continue stirring 1 hour.
Then 1 part of dropwise addition stearyl chloride (production of Shanghai Jing Chun biochemical technology limited liability company) continues to be stirred to react
Dehydrated alcohol (Sinopharm Chemical Reagent Co., Ltd.'s production) washing is added in 30min, filters and dry.Modified starch is made
1。
Modified starch 2；By cornstarch (production of Changchun great achievement corn development corporation, Ltd.) 100g and methyl acetate (traditional Chinese medicines
The production of chemical reagent Co., Ltd, group) 200 parts be blended at 60 DEG C, be thoroughly mixed 30min, be then added dropwise while stirring
50 parts of pyrroles's (Sinopharm Chemical Reagent Co., Ltd.'s production) after being added dropwise to complete, continues stirring 1 hour.
Then 100 parts of dropwise addition n-butyryl chloride (production of Shanghai Jing Chun biochemical technology limited liability company) continues to be stirred to react
Dehydrated alcohol (Sinopharm Chemical Reagent Co., Ltd.'s production) washing is added in 30min, filters and dry.Modified starch is made
2。
Modified starch 3: by tapioca (production of Shanghai Food Co., Ltd's today) 100g and butyl acetate (Chinese medicines group
The production of chemical reagent Co., Ltd) 150 parts be blended at 60 DEG C, be thoroughly mixed 30min, second two be then added dropwise while stirring
30 parts of amine (Sinopharm Chemical Reagent Co., Ltd.'s production) after being added dropwise to complete, continues stirring 1 hour.
Then 5 parts of dropwise addition stearyl chloride (production of Shanghai Jing Chun biochemical technology limited liability company) continues to be stirred to react
Dehydrated alcohol (Sinopharm Chemical Reagent Co., Ltd.'s production) washing is added in 30min, filters and dry.Modified starch is made
3。
Modified starch 4: by tapioca (production of Shanghai Food Co., Ltd's today) 100g and ethyl acetate (Chinese medicines group
The production of chemical reagent Co., Ltd) 200 parts be blended at 60 DEG C, be thoroughly mixed 30min, three second be then added dropwise while stirring
10 parts of amine (Sinopharm Chemical Reagent Co., Ltd.'s production) after being added dropwise to complete, continues stirring 1 hour.
Then n-butyryl chloride (production of Shanghai Jing Chun biochemical technology limited liability company) 10 parts of l are added dropwise to continue to be stirred to react
Dehydrated alcohol (Sinopharm Chemical Reagent Co., Ltd.'s production) washing is added in 30min, filters and dry.Modified starch is made
4。
Modified starch 5: by tapioca (production of Shanghai Food Co., Ltd's today) 100g and ethyl acetate (Chinese medicines group
The production of chemical reagent Co., Ltd) 100 parts and 100 parts of methyl acetate (Sinopharm Chemical Reagent Co., Ltd.'s production) is blended in
At 60 DEG C, it is thoroughly mixed 30min, then (Chinese medicines group chemical reagent is limited for dropwise addition triethylamine and ethylenediamine while stirring
Company's production) 10 parts of 1:1 blend, after being added dropwise to complete, continue stirring 1 hour.
Then lauroyl chloride (production of Shanghai Jing Chun biochemical technology limited liability company) 20 parts of l are added dropwise to continue to be stirred to react
Dehydrated alcohol (Sinopharm Chemical Reagent Co., Ltd.'s production) washing is added in 30min, filters and dry.Modified starch is made
5。
Modified starch 6: by cornstarch (production of Changchun great achievement corn development corporation, Ltd.) 100g and methyl acetate (traditional Chinese medicines
The production of chemical reagent Co., Ltd, group) 50 parts and 100 parts of butyl acetate (Sinopharm Chemical Reagent Co., Ltd.'s production) mixes
It closes at 60 DEG C, is thoroughly mixed 30min, then (Chinese medicines group chemical reagent has for dropwise addition pyrroles and triethylamine while stirring
The production of limit company) 18 parts of 1:1 blend, after being added dropwise to complete, continue stirring 1 hour.
Then 100 parts of dropwise addition n-butyryl chloride (production of Shanghai Jing Chun biochemical technology limited liability company) continues to be stirred to react
Dehydrated alcohol (Sinopharm Chemical Reagent Co., Ltd.'s production) washing is added in 30min, filters and dry.Modified starch is made
6。
Modified starch 7: by wheaten starch (production of Changchun great achievement corn development corporation, Ltd.) 100g and ethyl acetate (traditional Chinese medicines
The production of chemical reagent Co., Ltd, group) 200 parts and 100 parts of butyl acetate (Sinopharm Chemical Reagent Co., Ltd.'s production) mixes
It closes at 60 DEG C, is thoroughly mixed 30min, then (Chinese medicines group chemical reagent is limited for dropwise addition pyrroles and pyridine while stirring
Company's production) 18 parts of 1:1 blend, after being added dropwise to complete, continue stirring 1 hour.
Then 100 parts of dropwise addition caprylyl chloride (production of Shanghai Jing Chun biochemical technology limited liability company) continues to be stirred to react
Dehydrated alcohol (Sinopharm Chemical Reagent Co., Ltd.'s production) washing is added in 30min, filters and dry.Modified starch is made
7。
Embodiment 1
100 parts of modified starch 1 and 10 part polycaprolactones (PCL) (production of Shenzhen brilliance great achievement Co., Ltd) are mixed
It is even, pre-composition is placed in torque rheometer (Ha Bo Co., Ltd prepares RM-200 type), 10min is blended in 50rpm at 70 DEG C.
Blend is hot-forming by vulcanizing press, the sheet of 1 millimeters thick is obtained, and mark is cut into according to relevant criterion
Quasi- batten is used for Mechanics Performance Testing, and every test result is included in table 1, the water absorption rate in one week of test material, test result
It is included in table 1.
Embodiment 2
100 parts of modified starch 2 and 10 part polycaprolactones (PCL) (production of Shenzhen brilliance great achievement Co., Ltd) are mixed
It is even, pre-composition is placed in torque rheometer (Ha Bo Co., Ltd prepares RM-200 type), 10min is blended in 50rpm at 70 DEG C.
Blend is hot-forming by vulcanizing press, the sheet of 1 millimeters thick is obtained, and mark is cut into according to relevant criterion
Quasi- batten is used for Mechanics Performance Testing, and every test result is included in table 1, the water absorption rate in one week of test material, test result
It is included in table 1.
Embodiment 3
By 100 parts of modified starch 3 and 30 part polyadipates/butylene terephthalate (PBAT), (Shenzhen brilliance great achievement has
The production of limit company) it is uniformly mixed, pre-composition is placed in torque rheometer (Ha Bo Co., Ltd prepares RM-200 type), at 70 DEG C
10min is blended in 50rpm.
Blend is hot-forming by vulcanizing press, the sheet of 1 millimeters thick is obtained, and mark is cut into according to relevant criterion
Quasi- batten is used for Mechanics Performance Testing, and every test result is included in table 1, the water absorption rate in one week of test material, test result
It is included in table 1.
Embodiment 4
By 100 parts of modified starch 4 and 10 part polyadipates/butylene terephthalate (PBAT), (Shenzhen brilliance great achievement has
The production of limit company) it is uniformly mixed, pre-composition is placed in torque rheometer (Ha Bo Co., Ltd prepares RM-200 type), at 70 DEG C
10min is blended in 50rpm.
Blend is hot-forming by vulcanizing press, the sheet of 1 millimeters thick is obtained, and mark is cut into according to relevant criterion
Quasi- batten is used for Mechanics Performance Testing, and every test result is included in table 1, the water absorption rate in one week of test material, test result
It is included in table 1.
Embodiment 5
By 100 parts of modified starch 5 and 80 part poly butylene succinates (PBS) (production of Shenzhen brilliance great achievement Co., Ltd)
It is uniformly mixed, pre-composition is placed in torque rheometer (Ha Bo Co., Ltd prepares RM-200 type), 50rpm is blended at 70 DEG C
10min。
Blend is hot-forming by vulcanizing press, the sheet of 1 millimeters thick is obtained, and mark is cut into according to relevant criterion
Quasi- batten is used for Mechanics Performance Testing, and every test result is included in table 2, the water absorption rate in one week of test material, test result
It is included in table 3.
Embodiment 6
100 parts of modified starch 6 and 100 part poly-β-hydroxybutyric acids (PHB) (production of Shenzhen brilliance great achievement Co., Ltd) are mixed
Uniformly, pre-composition is placed in torque rheometer (Ha Bo Co., Ltd prepares RM-200 type), 10min is blended in 50rpm at 70 DEG C.
Blend is hot-forming by vulcanizing press, the sheet of 1 millimeters thick is obtained, and mark is cut into according to relevant criterion
Quasi- batten is used for Mechanics Performance Testing, and every test result is included in table 1, the water absorption rate in one week of test material, test result
It is included in table 1.
Embodiment 7
By 100 portions of modified starches 7 and 100 parts of polyhydroxyalkanoate (PHA) (production of Shenzhen brilliance great achievement Co., Ltd)
It is uniformly mixed, pre-composition is placed in torque rheometer (Ha Bo Co., Ltd prepares RM-200 type), 50rpm is blended at 70 DEG C
10min。
Blend is hot-forming by vulcanizing press, the sheet of 1 millimeters thick is obtained, and mark is cut into according to relevant criterion
Quasi- batten is used for Mechanics Performance Testing, and every test result is included in table 1, the water absorption rate in one week of test material, test result
It is included in table 1.
The performance of table 1 embodiment and comparative example
The starch-based bio composite material obtained through the invention has biomass compared with current conventional thermoplastic's material
The advantages that content is high, part biological is degradable, resilience is good, can satisfy the basic requirement of material.By to starch into
Row is modified, and improves the hydrophobicity of starch molecule and the compatibility with polyester material, thus can be the high-content of starch the case where
Under, it is blended with polyester material.Compare comparative example 1 and embodiment 1,2, comparative example 2 and embodiment 3, comparative example 4 and embodiment
6 data, it can be seen that starch-based bio composite material tensile strength and elongation at break obtained in embodiment obtain
It improves, while comparing common starch filled method, the water absorption rate of composite material of the invention substantially reduces.Therefore, of the invention
Content is a breakthrough to traditional starch sill in performance.Simultaneously because not deposited in the present invention without using plasticizer
It will not be lost rapidly in the mechanical property of the safety problem of the migration of plasticizer, while material.
Claims (5)
1. a kind of starch-based composite material, it is characterised in that:
The composite material is blended by the modified starch and polyester melt of parts by weight meter,
100 parts by weight of modified starch, polyester 10 to less than 100 parts by weight；
The general structure of the modified starch are as follows:
Wherein St is starch molecule, and R group is alkyl (CnH2n+1), alkenyl (CnH2n), phenyl (CnHN~1At least one of),
In, n=2~18；
The modified starch is prepared by the following components of parts by weight meter:
100 parts of native starch, 0~200 part of solvent, 10~50 parts of catalyst, 1~50 part of modifying agent；
The native starch be selected from cornstarch, tapioca, starch from sweet potato, potato starch, wheat starch, bean starch or
At least one of sorghum starch；
The solvent is selected from at least one of ethyl acetate, butyl acetate, methyl acetate；
The catalyst is selected from at least one of organic bases or polyamine；
The modifying agent is acyl chloride；
The modified starch is by including that the method for following steps is prepared:
(1) catalytic pretreatment of starch: solvent is added to native starch or native starch, dropwise addition catalysis in starch suspension is made
Then agent is stirred 0.5~3 hour at 10 DEG C~60 DEG C；
(2) modification of starch: being added dropwise modifying agent while stirring, and anhydrous second is added after stirring 0.5~3 hour at 10 DEG C~60 DEG C
Alcohol washing filters, the modified starch is made after drying；
The polyester is degradable polyester.
2. starch-based composite material as described in claim 1, it is characterised in that:
100 parts of native starch, 150~200 parts of solvent, 10~30 parts of catalyst, 1~20 part of modifying agent.
3. starch-based composite material as described in claim 1, it is characterised in that:
The catalyst is selected from least one of pyridine, pyrroles, ethylenediamine and triethylamine；
The modifying agent is acryloyl chloride.
4. a kind of preparation method of the starch-based composite material as described in one of claims 1 to 3, it is characterised in that:
The starch-based composite material is made by the dosage melt blending in the component.
5. the preparation method of starch-based composite material as claimed in claim 4, it is characterised in that:
Melt blending temperature is 60~230 DEG C.
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| CN107513245B (en) * | 2016-06-16 | 2019-12-20 | 江南大学 | Modified starch toughened polymethyl methacrylate composite material and preparation method thereof |
| CN107513252B (en) * | 2016-06-16 | 2020-04-24 | 江南大学 | Toughened thermosetting composite material based on modified starch and preparation method thereof |
| CN107513246B (en) * | 2016-06-16 | 2020-04-24 | 江南大学 | Toughening thermoplastic composite material based on modified starch and preparation method thereof |
| CN107513258A (en) * | 2016-06-16 | 2017-12-26 | 江南大学 | A kind of high-toughness high-strength starch composite material and preparation method |
| CN108586824A (en) * | 2018-05-22 | 2018-09-28 | 上海顶贤贸易有限公司 | A kind of complete-degradable plastic and preparation method thereof |
| CN110396293B (en) * | 2019-07-08 | 2021-10-08 | 江南大学 | Easily-formed three-layer core-shell particle toughened polymer composite material and preparation method thereof |
| CN113321905B (en) * | 2021-06-22 | 2022-04-08 | 江南大学 | Modified starch/poly (butylene succinate) composite material |
| CN115448988A (en) * | 2022-09-05 | 2022-12-09 | 河南新孚望新材料科技有限公司 | Method for efficiently preparing acetate high-amylose corn starch |
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